Reacción #524944

ord-75972cc5fec742c895ee16a4f27e5f2d

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONA mixture containing 8.2 g
  2. 2
    Concentraciónconcentrated in vacuo to dryness
  3. 3
    Otrothe solid collected
  4. 4
    workup.DISSOLUTIONThe solid was dissolved
  5. 5
    workup.ADDITIONthe hot solution treated with decolorizing charcoal
  6. 6
    Filtraciónfiltered
  7. 7
    Temperaturato cool
  8. 8
    workup.ADDITIONsaturated with gaseous hydrogen chloride, ether was added to turbidity
  9. 9
    OtroThe separated solid was collected
  10. 10
    Otrodried in vacuo at 80° C.
  11. 11
    Otroto yield 7.4 g

Procedimiento

A mixture containing 8.2 g. of 4-chloro-6-methyl-2-(4-pyridinyl)pyrimidine, 8.7 g. of diethylamine hydrochloride, 100 ml. of ethanol, 6 g. of potassium carbonate and 10 ml. of water was refluxed with stirring for eight hours and then concentrated in vacuo to dryness. The residue was swirled in water and the solid collected. The solid was dissolved in boiling isopropyl alcohol, the hot solution treated with decolorizing charcoal and filtered, and the hot filtrate allowed to cool. The filtrate was then saturated with gaseous hydrogen chloride, ether was added to turbidity and the mixture was allowed to stand. The separated solid was collected and dried in vacuo at 80° C. to yield 7.4 g. of N,N-diethyl-6-methyl-2-(4-pyridinyl)-4-pyrimidinamine dihydrochloride, m.p. 205°-208° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04032523uspto-grants-1977_06